CN109980201A - A kind of preparation method and application of ternary cathode material of lithium ion battery - Google Patents
A kind of preparation method and application of ternary cathode material of lithium ion battery Download PDFInfo
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Abstract
The invention discloses a kind of preparation methods of ternary cathode material of lithium ion battery: utilizing DC installation, it is electrolysed the ni mn co alloy working electrode being placed in soluble inorganic salt electrolyte solution, electrolysate is by being centrifuged, washing, being dried to obtain ternary anode material precursor Ni1‑x‑yCoxMny(OH)2, then with calcining after lithium source mixed grinding to get LiNi1‑x‑yCoxMnyO2Tertiary cathode material, wherein x=0.1~0.4, y=0.1~0.4.Operation of the present invention is simple, and yield is high, low production cost, the substance containing pollution environment toxic to human body will not be generated in preparation process, and electrolyte can be reused, and has advantage that is apparent environmentally protective and economizing on resources.
Description
Technical field
The invention belongs to anode material for lithium-ion batteries technical fields, and in particular to a kind of lithium ion battery tertiary cathode material
The preparation method and application of material.
Background technique
Lithium ion battery has high specific energy, good cycle and the advantages such as pollution is small extensive as secondary cell
It applies on various energy storage devices.Since positive electrode is material the most key in generally acknowledged lithium ion battery, performance is good
It is bad to directly affect the energy storage density of battery, cycle life, safety etc. performance, so its development also most merits attention.Mesh
The anode material for lithium ion battery of preceding industrialization mainly has cobalt acid lithium, modified lithium manganate, ternary material, LiFePO4.Its
In, nickel-cobalt-manganese ternary material is a kind of Olivine-type Cathode Material in Li-ion Batteries developed in recent years, has capacity height, stable circulation
Property the important advantages such as good, moderate cost, since this kind of material can effectively overcome simultaneously, cobalt acid lithium material cost is excessively high, LiMn2O4
The problems such as stability of material is not high, LiFePO4 capacity is low has been achieved with successful application in the battery, and obtains using scale
Rapid development is arrived.
Currently, the preparation method of ternary material precursor is mainly wet chemistry method, specially solution is co-precipitated gentle gelling
Glue method.Solution co-precipitation needs strong alkali environment, and the processing of waste liquid can bring certain environmental pressure.Gas sol-gel technical process
Complexity can not be applied on a large scale.The synthetic method of ternary material mainly have high temperature solid-state method, coprecipitation, spray drying process,
Hydro-thermal method, sol-gal process etc..Wherein hydro-thermal method and sol-gal process are not suitable for industrializing due to being limited by preparation method
Production.High temperature solid-state method is most common in powder preparation, and advantage is that equipment requirement is not high, operating procedure is simple, easily controllable,
But raw material mixes uneven and the unequal factors affect material of distribution of particles performance.Simultaneous reactions overlong time, energy consumption compared with
Greatly, it is difficult to control stoichiometric ratio, miscellaneous phase easily generated, it is not very stable for causing the chemical property of product.It is spray-dried legal system
Standby material is visibly homogeneous, and particle is subtle, has advantage in the stoichiometric composition of material, pattern and particle diameter distribution, and
Can with automation control, can continuous production, preparative capacibility is strong.This method temporarily can not the major defect of large-scale application be work
Skill process is complicated, has sizable difficulty in instrument and equipment design, actual process operation and control.Coprecipitation is current
The preparation process that industrialized production ternary material generallys use.The particle size that coprecipitation obtains is small and narrow distribution range, but
Product is relatively high to the requirement of the conditions such as precipitation temperature, solution concentration, pH value, stirring intensity and sintering temperature, and due to each
The settling rate etc. of component has differences, and the uniformity of product is not ideal enough.In addition, subsequent liquid waste processing step, can also increase
Add production cost.
Summary of the invention
In order to overcome the shortcomings in the prior art, the present invention provide a kind of easy to operate, yield is high, environmentally protective lithium from
The preparation method of sub- battery tertiary cathode material.
In order to achieve the above technical purposes, the present invention adopts the following technical scheme:
A kind of preparation method of ternary cathode material of lithium ion battery: utilizing DC installation, and electrolysis is placed in soluble nothing
Ni mn co alloy working electrode in machine salt electrolyte solution, electrolysate is by being centrifuged, washing, being dried to obtain tertiary cathode material
Material precursor Ni1-x-yCoxMny(OH)2, then with calcining after lithium source mixed grinding to get LiNi1-x-yCoxMnyO2Tertiary cathode material
Expect, wherein x=0.1~0.4, y=0.1~0.4.
Preferably, the soluble inorganic salt include soluble villaumite, it is soluble sulphate, soluble nitrate, solvable
At least one of acid carbonate；The solubility villaumite includes sodium chloride, potassium chloride, calcium chloride, ammonium chloride, manganese chloride, chlorine
Change lead, magnesium chloride, iron chloride, at least one of aluminium chloride；The soluble sulphate includes sodium sulphate, ammonium sulfate, sulfuric acid
Potassium, magnesium sulfate, manganese sulfate, at least one of aluminum sulfate；The soluble nitrate includes sodium nitrate, potassium nitrate, ammonium nitrate,
Calcium nitrate, plumbi nitras, manganese nitrate, at least one of magnesium nitrate；The soluble carbonate salt includes sodium carbonate, ammonium carbonate, carbon
Sour potassium, sodium bicarbonate, saleratus, at least one of ammonium hydrogen carbonate.
Preferably, the concentration of the soluble inorganic salt electrolyte solution be 0.05~5.0mol/L, more preferably 0.1~
4.5mol/L。
Preferably, the voltage that the DC installation applies is 2~50V, more preferably 5~40V.
Preferably, the construction of the ni mn co alloy working electrode is nickel cobalt manganese alloy/nickel cobalt manganese alloy working electrode, nickel
Cobalt manganese alloy/platinum working electrode, nickel cobalt manganese alloy/graphite rod working electrode, nickel cobalt manganese alloy/nickel working electrode, nickel cobalt manganese are closed
At least one of gold/manganese and nickel cobalt manganese alloy/cobalt working electrode.
Preferably, the molar ratio of the ternary anode material precursor and lithium source is 1:0.2~5.
Preferably, the lithium source includes at least one of lithium chloride, lithium acetate, lithium carbonate, lithium hydroxide and lithium bromide.
Preferably, the calcination temperature be 300~1100 DEG C, more preferably 550~950 DEG C, the calcination time be 2~
24h。
Preferably, heating rate is 1~25 DEG C/min, more preferably 5~20 DEG C/min in the calcination process.
The ternary cathode material of lithium ion battery that preparation method of the present invention is prepared.
The application of ternary cathode material of lithium ion battery of the present invention: LiNi1-x-yCoxMnyO2As positive electrode,
N- dimethyl pyrrolidone is dispersed in after mixing with polyvinylidene fluoride, super carbon black 60~90:5 in mass ratio~20:5~20
In, be coated on aluminium foil after being uniformly mixed, 60~120 DEG C of vacuum drying obtain positive pole aluminium foil piece, after cutting with lithium piece group
Dress up half-cell.
The method that direct current electrochemistry of the present invention prepares presoma and tertiary cathode material, specific steps are such as
Under:
(1) by a certain amount of inorganic salts be added 100~1000mL distilled water in it is agitated obtain concentration be 0.05~
The inorganic salts dispersion liquid of 5.0mol/L, as electrolyte solution；
(2) ni mn co alloy working electrode is immersed in the electrolyte solution of above-mentioned steps (1), and by DC voltage
It is set as 2~50V；
(3) when electrode surface does not have substance to fall off, electrolysis terminates, and is centrifuged to electrolysate, uses distilled water respectively
Ternary anode material precursor Ni is obtained with ethanol washing 5 times, dry collect1-x-yCoxMny(OH)2, temperature is 50~100 DEG C,
Drying time is 8~48h；
(4) ternary anode material precursor of above-mentioned steps (3) is equal by the molar ratio ground and mixed of 1:0.2-5 with lithium source
It is even, it places it in tube furnace, heating rate is 1-20 DEG C/min, in air, 300~1100 DEG C of calcinings 2~obtain three for 24 hours
First positive electrode.
By LiNi1-x-yCoxMnyO2Tertiary cathode material is applied in lithium ion battery, the specific steps are as follows:
(1) by LiNi1-x-yCoxMnyO2Powder and super carbon black and polyvinylidene fluoride binder press 60~90:5~20:5
~20 mass ratio mixing, is added suitable N- dimethyl pyrrolidone and stirs to form suspension, be then equably coated in aluminium foil
On, 60~120 DEG C of vacuum drying obtain positive pole aluminium foil piece, and working electrode is used as after cutting.Lithium metal is used as to electrode,
Celgard 2400 is used as diaphragm, 1.0mol/L LiPF6/ EC+DMC (volume ratio 1:1) is used as electrolyte, in argon gas protection
Half-cell is assembled into glove box.
(2) chemical property of above-mentioned (1) assembling half-cell is tested using Arbin battery cycler (BT2000).
Compared with the prior art, technical solution of the present invention bring advantageous effects:
1) method of present invention preparation ternary anode material precursor is to pass through direct current using nickel cobalt manganese alloy as working electrode
Prepared by electricity electrolysis inorganic salt solution, the substance containing pollution environment toxic to human body, and electricity will not be generated in electrolytic process
Solution liquid can be reused, and compared with the prior art, have advantage that is apparent environmentally protective and economizing on resources.
2) present invention preparation ternary anode material precursor uses direct current electrochemical method, solid with the high temperature of the prior art
The method of the preparation ternary anode material precursor such as Xiang Fa, coprecipitation, spray drying process, hydro-thermal method, sol-gal process is compared,
With the characteristics of easy to operate, yield is high, low production cost, be conducive to industrialized production.
3) present invention has that partial size is small, particle with ternary anode material precursor prepared by direct current electrochemical method for the first time
It is evenly distributed, the advantage of purity is high, the tertiary cathode material LiNi that it is used to prepare1-x-yCoxMnyO2It applies in lithium-ion electric
Chi Zhong has good chemical property.
Detailed description of the invention
Fig. 1 is Ni obtained in embodiment 11/3Co1/3Mn1/3(OH)2Presoma and LiNi1/3Co1/3Mn1/3O2Positive electrode
XRD diagram；
Fig. 2 is Ni obtained in embodiment 11/3Co1/3Mn1/3(OH)2The scanning electron microscope (SEM) photograph of presoma；
Fig. 3 is LiNi obtained in embodiment 11/3Co1/3Mn1/3O2The scanning electron microscope (SEM) photograph of positive electrode；
Fig. 4 is LiNi obtained in embodiment 11/3Co1/3Mn1/3O2The cycle performance figure of positive electrode.
Fig. 5 is Ni obtained in embodiment 20.6Co0.2Mn0.2(OH)2Presoma and LiNi0.6Co0.2Mn0.2O2Positive electrode
XRD diagram；
Fig. 6 is LiNi obtained in embodiment 20.6Co0.2Mn0.2O2The cycle performance figure of positive electrode.
Specific embodiment
Following embodiment is in order to which the present invention is explained in greater detail, these embodiments do not form any restrictions to the present invention,
The present invention can be implemented by formula either described in summary of the invention.
Embodiment 1
(1) direct current electrochemical method prepares Ni1/3Co1/3Mn1/3(OH)2Presoma and LiNi1/3Co1/3Mn1/3O2Ternary
Positive electrode
The potassium nitrate electricity of 300mL 2mol/L is immersed in using ni mn co alloy (111)/ni mn co alloy as working electrode
In electrolyte solution.Then 10V is set by DC voltage to be electrolysed.After to be electrolysed, electrolysate is centrifuged,
And distilled water and ethanol washing 5 times are used respectively, in 60 DEG C of dry collections.By the electrolysate after drying with lithium carbonate by 1.2
Molar ratio ground and mixed is uniform, places it in tube furnace, and in air, 800 DEG C of calcining 12h, heating rate is 10 DEG C/min,
It is collected after cooling spare.
(2)LiNi1/3Co1/3Mn1/3O2Application of the positive electrode in lithium ion battery
By LiNi1/3Co1/3Mn1/3O2Powder and active carbon and polyvinylidene fluoride binder press the mass ratio of 70:15:15
Mixing, is added suitable N- dimethyl pyrrolidone and stirs to form suspension, be then equably coated on aluminium foil, and 80 DEG C of vacuum are dry
It is dry to obtain positive pole aluminium foil piece, working electrode is used as after cutting.Lithium metal is used as to electrode, and Celgard 2400 is used as diaphragm,
1.0mol/L LiPF6/ EC+DMC (volume ratio 1:1) is used as electrolyte, is assembled into half-cell in the glove box of argon gas protection.
The chemical property of above-mentioned assembling half-cell is tested using Arbin battery cycler (BT2000).
Fig. 1 is Ni1/3Co1/3Mn1/3(OH)2Presoma and LiNi1/3Co1/3Mn1/3O2The XRD diagram of positive electrode, it can be seen that
Ni1/3Co1/3Mn1/3(OH)2Presoma and Ni (OH)2Diffraction maximum is corresponding, shows part Ni2+By Co2+、Mn2+Replace.LiNi1/ 3Co1/3Mn1/3O2(006) of positive electrode/(102) and (108)/(110) diffraction maximum separate well, show the positive material of preparation
Material has good crystal form and hexagon lamellar structure.Fig. 2 is Ni1/3Co1/3Mn1/3(OH)2The scanning electron microscopic picture of presoma,
It can be seen that having the advantages that partial size is small, is evenly distributed using presoma prepared by electrochemistry.Fig. 3 is LiNi1/3Co1/3Mn1/3O2
The scanning electron microscopic picture of positive electrode, it can be seen that the tertiary cathode material partial size using the precursor preparation of electrochemistry preparation is small
(1 μm of ﹤), distribution is relatively narrow.Fig. 4 is LiNi1/3Co1/3Mn1/3O2The cycle performance figure of positive electrode, coulombic efficiency reaches for the first time
To 90.1%, at 0.1C (17mAh/g), first discharge specific capacity shows to prepare using electrochemistry up to 181.8mAh/g
Precursor preparation tertiary cathode material apply lithium ion battery have excellent chemical property.
Embodiment 2
(1) direct current electrochemical method prepares Ni0.6Co0.2Mn0.2(OH)2Presoma and LiNi0.6Co0.2Mn0.2O2Ternary
Positive electrode
It is the sodium sulphate electrolyte solution that working electrode is immersed in 300mL 0.5mol/L by ni mn co alloy (622)/platinum
In.Then 8V is set by DC voltage to be electrolysed.After to be electrolysed, electrolysate is centrifuged, and is used respectively
Distilled water and ethanol washing 5 times dry are collected at 80 DEG C.By after drying electrolysate and lithium hydroxide press 0.8 molar ratio
Ground and mixed is uniform, places it in tube furnace, and in air, 850 DEG C of calcining 16h, heating rate is 5 DEG C/min, after cooling
It collects spare.
(2)LiNi0.6Co0.2Mn0.2O2Application of the positive electrode in lithium ion battery
By LiNi0.6Co0.2Mn0.2O2Powder and active carbon and polyvinylidene fluoride binder press the mass ratio of 80:10:10
Mixing, is added suitable N- dimethyl pyrrolidone and stirs to form suspension, be then equably coated on aluminium foil, and 90 DEG C of vacuum are dry
It is dry to obtain positive pole aluminium foil piece, working electrode is used as after cutting.Lithium metal is used as to electrode, and Celgard 2400 is used as diaphragm,
1.0mol/L LiPF6/ EC+DMC (volume ratio 1:1) is used as electrolyte, is assembled into half-cell in the glove box of argon gas protection.
The chemical property of above-mentioned assembling half-cell is tested using Arbin battery cycler (BT2000).
Fig. 5 is Ni0.6Co0.2Mn0.2(OH)2Presoma and LiNi0.6Co0.2Mn0.2O2The XRD diagram of positive electrode,
Ni0.6Co0.2Mn0.2(OH)2Presoma is shown and Ni (OH)2Corresponding diffraction maximum shows part Ni2+By Co2+、Mn2+Success
Replace.LiNi0.6Co0.2Mn0.2O2(006) of positive electrode/(102) and (108)/(110) diffraction maximum successfully separate, and
I003/I104Value be 1.5214 (are greater than 1.2), show that the positive electrode obtained has preferable crystalline structure.Fig. 6 is
LiNi0.6Co0.2Mn0.2O2The cycle performance figure of positive electrode, coulombic efficiency has reached 89.4% for the first time, at 0.1C (17mAh/g)
Under, first discharge specific capacity is showing precursor preparation (622) the system ternary obtained using electrochemistry just up to 197.8mAh/g
Pole material, which is applied, has excellent chemical property in lithium ion battery.
Embodiment 3
(1) direct current electrochemical method prepares Ni1/3Co1/3Mn1/3(OH)2Presoma and LiNi1/3Co1/3Mn1/3O2Ternary
Positive electrode
The sodium chloride electrolysis matter solution of 500mL 1mol/L is immersed in using ni mn co alloy (111)/nickel as working electrode
In.Then 15V is set by DC voltage to be electrolysed.After to be electrolysed, electrolysate is centrifuged, and is used respectively
Distilled water and ethanol washing 5 times dry are collected at 80 DEG C.By after drying electrolysate and lithium carbonate grind by 1.05 molar ratio
Mill is uniformly mixed, and is placed it in tube furnace, and in air, 900 DEG C of calcining 18h, heating rate is 4 DEG C/min, is received after cooling
Collect spare.
(2)LiNi1/3Co1/3Mn1/3O2Application of the positive electrode in lithium ion battery
By LiNi1/3Co1/3Mn1/3O2Powder and active carbon and polyvinylidene fluoride binder press the mass ratio of 70:20:10
Mixing, is added suitable N- dimethyl pyrrolidone and stirs to form suspension, be then equably coated on aluminium foil, and 80 DEG C of vacuum are dry
It is dry to obtain positive pole aluminium foil piece, working electrode is used as after cutting.Lithium metal is used as to electrode, and Celgard 2400 is used as diaphragm,
1.0mol/L LiPF6/ EC+DMC (volume ratio 1:1) is used as electrolyte, is assembled into half-cell in the glove box of argon gas protection.
The chemical property of above-mentioned assembling half-cell is tested using Arbin battery cycler (BT2000).
Embodiment 4
(1) direct current electrochemical method prepares Ni0.6Co0.2Mn0.2(OH)2Presoma and LiNi0.6Co0.2Mn0.2O2Ternary
Positive electrode
The sodium carbonate electrolyte for being immersed in 800mL 0.6mol/L using ni mn co alloy (622)/platinum as working electrode is molten
In liquid.Then 16V is set by DC voltage to be electrolysed.After to be electrolysed, electrolysate is centrifuged, and respectively
With distilled water and ethanol washing 5 times, collected in 70 DEG C of dryings.By after drying electrolysate and lithium carbonate press 1.6 molar ratio
Ground and mixed is uniform, places it in tube furnace, and in air, 880 DEG C of calcining 20h, heating rate is 15 DEG C/min, after cooling
It collects spare.
(2)LiNi0.6Co0.2Mn0.2O2Application of the positive electrode in lithium ion battery
By LiNi0.6Co0.2Mn0.2O2Powder and active carbon and polyvinylidene fluoride binder are mixed by the mass ratio of 80:15:5
It closes, suitable N- dimethyl pyrrolidone is added and stirs to form suspension, is then equably coated on aluminium foil, 80 DEG C of vacuum drying
Positive pole aluminium foil piece is obtained, working electrode is used as after cutting.Lithium metal is used as to electrode, and Celgard 2400 is used as diaphragm,
1.0mol/L LiPF6/ EC+DMC (volume ratio 1:1) is used as electrolyte, is assembled into half-cell in the glove box of argon gas protection.
The chemical property of above-mentioned assembling half-cell is tested using Arbin battery cycler (BT2000).
Claims (11)
1. a kind of preparation method of ternary cathode material of lithium ion battery, it is characterised in that: utilize DC installation, electrolysis is placed in
Ni mn co alloy working electrode in soluble inorganic salt electrolyte solution, electrolysate is by being centrifuged, washing, being dried to obtain three
First positive electrode material precursor Ni1-x-yCoxMny(OH)2, then with calcining after lithium source mixed grinding to get LiNi1-x-yCoxMnyO2Three
First positive electrode, wherein x=0.1~0.4, y=0.1~0.4.
2. the preparation method of ternary cathode material of lithium ion battery according to claim 1, it is characterised in that: described solvable
Property inorganic salts include at least one of soluble villaumite, soluble sulphate, soluble nitrate, soluble carbonate salt；Institute
Stating soluble villaumite includes sodium chloride, potassium chloride, calcium chloride, ammonium chloride, manganese chloride, lead chloride, magnesium chloride, iron chloride, chlorination
At least one of aluminium；The soluble sulphate includes sodium sulphate, ammonium sulfate, potassium sulfate, magnesium sulfate, manganese sulfate, aluminum sulfate
At least one of；The soluble nitrate includes sodium nitrate, potassium nitrate, ammonium nitrate, calcium nitrate, plumbi nitras, manganese nitrate, nitre
At least one of sour magnesium；The soluble carbonate salt includes sodium carbonate, ammonium carbonate, potassium carbonate, sodium bicarbonate, saleratus,
At least one of ammonium hydrogen carbonate.
3. the preparation method of ternary cathode material of lithium ion battery according to claim 1, it is characterised in that: described solvable
Property inorganic salts electrolyte solution concentration be 0.05~5.0mol/L.
4. the preparation method of ternary cathode material of lithium ion battery according to claim 1, it is characterised in that: the direct current
The voltage that electric equipment applies is 2~50V.
5. the preparation method of ternary cathode material of lithium ion battery according to claim 1, it is characterised in that: the nickel manganese
The construction of cobalt alloy working electrode is nickel cobalt manganese alloy/nickel cobalt manganese alloy working electrode, nickel cobalt manganese alloy/platinum working electrode, nickel
Cobalt manganese alloy/graphite rod working electrode, nickel cobalt manganese alloy/nickel working electrode, nickel cobalt manganese alloy/manganese and nickel cobalt manganese alloy/cobalt work
Make at least one of electrode.
6. the preparation method of ternary cathode material of lithium ion battery according to claim 1, it is characterised in that: the ternary
The molar ratio of positive electrode material precursor and lithium source is 1:0.2~5.
7. the preparation method of ternary cathode material of lithium ion battery according to claim 1, it is characterised in that: the lithium
Source includes at least one of lithium chloride, lithium acetate, lithium carbonate, lithium hydroxide and lithium bromide.
8. the preparation method of ternary cathode material of lithium ion battery according to claim 1, it is characterised in that: the calcining
Temperature be 300~1100 DEG C, calcination time be 2~for 24 hours,
9. the preparation method of ternary cathode material of lithium ion battery according to claim 1, it is characterised in that: the calcining
Heating rate is 1~25 DEG C/min in the process.
10. ternary cathode material of lithium ion battery made from the described in any item preparation methods of claim 1-9.
11. the application of ternary cathode material of lithium ion battery described in any one of claim 10: LiNi1-x-yCoxMnyO2As positive material
Material, is dispersed in N- dimethyl pyrrole after mixing with polyvinylidene fluoride, super carbon black 60~90:5 in mass ratio~20:5~20
In alkanone, be coated on aluminium foil after being uniformly mixed, 60~120 DEG C of vacuum drying obtain positive pole aluminium foil piece, after cutting with lithium
Piece is assembled into half-cell.
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| CN111725499A (en) * | 2020-06-29 | 2020-09-29 | 天津理工大学 | Method for preparing lithium battery cathode material NCM811 by using co-precipitation method with electrolytic method |
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| CN103280572A (en) * | 2013-05-27 | 2013-09-04 | 华南师范大学 | Ternary positive pole material of lithium ion battery and preparation method of ternary positive pole material |
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| CN103280572A (en) * | 2013-05-27 | 2013-09-04 | 华南师范大学 | Ternary positive pole material of lithium ion battery and preparation method of ternary positive pole material |
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| CN111725499A (en) * | 2020-06-29 | 2020-09-29 | 天津理工大学 | Method for preparing lithium battery cathode material NCM811 by using co-precipitation method with electrolytic method |
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